CN111302773A - Preparation method of mullite porous ceramic - Google Patents
Preparation method of mullite porous ceramic Download PDFInfo
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Abstract
The invention belongs to the technical field of ceramic materials, and particularly relates to a preparation method of mullite porous ceramic. The invention aims to solve the technical problem of providing a preparation method of mullite porous ceramic, which comprises the following steps: uniformly mixing quartz sand powder, special-grade bauxite powder, a bonding agent, a mineralizer and a pore-forming agent, adding water, and uniformly mixing to obtain a semi-dry material; pouring the semi-dry material into a mould to form a semi-finished product, and calcining the semi-finished product to obtain mullite porous ceramic; the binding agent is aluminate cement, and the mineralizer is titanium dioxide. The mullite porous ceramic prepared by the method has good performance.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to a preparation method of mullite porous ceramic.
Background
The composition of mullite is 3Al2O3·2SiO2The mullite belongs to a double-chain aluminosilicate mineral of an orthorhombic system, and the crystal structure of the mullite is formed by disordered arrangement of most basic silicon-oxygen tetrahedral mechanism units and aluminum-oxygen tetrahedral mechanism units along a c axis to form double chains, and the double chains are connected by aluminum-oxygen octahedrons in a common vertex angle and common edge mode. Because the mullite ceramic has good performances in the aspects of high-temperature stability, high-temperature mechanical property, high-temperature creep resistance, chemical stability, thermal expansibility and insulativity, the mullite is widely used for high-temperature structural materials and functional materials and is applied to the fields of national defense, high-tech civil use, industry and the like. Such as: high temperature refractory materials, electronic materials, chemical materials, optical materials, high temperature structural materials, and the like.
The porous mullite ceramic is a mullite ceramic material which takes mullite ceramic as a substrate and is formed by arranging a plurality of air holes in space in various modes. The porous mullite ceramic has the characteristics of uniform thermal expansion, high refractoriness under load, excellent thermal shock resistance, high hardness, small high-temperature creep value, good chemical corrosion resistance and the like, and is developed rapidly as a novel material. Currently, porous mullite ceramics are used in gas sensors, catalyst supports, hot gas or molten metal filters, and high temperature refractory insulation. As a catalyst carrier, compared with other catalyst carriers, the porous mullite ceramic has great advantages in the aspects of high temperature resistance, corrosion resistance, no pollution to the catalyst, low cost and the like.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of mullite porous ceramic. The preparation method comprises the following steps: uniformly mixing quartz sand powder, special-grade bauxite powder, a bonding agent, a mineralizer and a pore-forming agent, adding water, and uniformly mixing to obtain a semi-dry material; pouring the semi-dry material into a mould to form a semi-finished product, and calcining the semi-finished product to obtain mullite porous ceramic; the binding agent is aluminate cement, and the mineralizer is titanium dioxide.
In the preparation method of the mullite porous ceramic, the pore-forming agent is at least one of silicon carbide, starch, graphite powder, wood chips or plant fibers.
Wherein, in the preparation method of the mullite porous ceramic, SiO in the quartz sand powder2≥98％。
Wherein, in the preparation method of the mullite porous ceramic, Al in the special-grade bauxite powder2O3≥85％。
In the preparation method of the mullite porous ceramic, the granularity of the quartz sand powder is less than or equal to 0.088 mm.
In the preparation method of the mullite porous ceramic, the granularity of the special-grade bauxite powder is less than or equal to 0.088 mm.
In the preparation method of the mullite porous ceramic, the addition amount of the aluminate cement is 5-8% of the total mass of the quartz sand powder and the special-grade bauxite powder.
In the preparation method of the mullite porous ceramic, the addition amount of the titanium dioxide is 5-8% of the total mass of the quartz sand powder and the special-grade bauxite powder.
In the preparation method of the mullite porous ceramic, the addition amount of the pore-forming agent is 5-8% of the total mass of the quartz sand powder and the special-grade bauxite powder.
In the preparation method of the mullite porous ceramic, the addition amount of water is 6-9% of the total mass of the quartz sand powder and the special-grade bauxite powder.
In the preparation method of the mullite porous ceramic, the water content of each raw material is below 2%.
In the preparation method of the mullite porous ceramic, the forming pressure is 15-25 MPa, and the pressure is maintained for 5-10 s.
In the preparation method of the mullite porous ceramic, the calcining temperature is 1250-1350 ℃, and the time is 3-6 hours.
Preferably, in the preparation method of the mullite porous ceramic, the calcining temperature and time are 1300 ℃ multiplied by 4 h.
The invention selects the high-quality raw materials of the special-grade alumina powder and the quartz sand, can reduce the carrying amount of impurities, improves the sintering effect of the mullite porous ceramic, and is favorable for improving the bending strength of the mullite porous ceramic; by selecting titanium dioxide as a mineralizer, the titanium dioxide has a good mineralization effect, can reduce the sintering temperature of the mullite porous ceramic, and can further improve the bending strength of the mullite porous ceramic; aluminate cement is selected as a binding agent, the aluminate cement has hydration characteristics, the strength of a die-out sample can be improved, the qualification rate of a semi-finished product is improved, a small amount of calcium oxide contained in the aluminate cement can play a role of a mineralizer, the sintering temperature of the mullite porous ceramic can be reduced to a certain extent, and the bending strength of the mullite porous ceramic is improved; the pore former is selected primarily with regard to production costs.
Detailed Description
1. Detecting moisture
The water content of the raw materials used for analysis and detection is too much, the caking and bonding phenomena in the mixing process can be caused, the water content exceeds 2 percent, the raw materials are dried, and the mixing uniformity is ensured.
2. Ingredients
According to mullite chemical formula 3Al2O3-2SiO2Calculating the theoretical required SiO228.2％、Al2O371.8% and SiO contained in the selected raw material2、Al2O3Weighing and proportioning quartz sand powder and special-grade bauxite powder which meet the requirements of a mullite chemical formula, and additionally adding a bonding agent, a mineralizer and a pore-forming agent. When the granularity of the quartz sand powder and the special-grade bauxite powder is larger, the quartz sand powder and the special-grade bauxite powder are ground by a ball mill.
3. Mixing
The weighed quartz sand powder, the special-grade bauxite powder, the bonding agent, the pore-forming agent and the mineralizing agent are conveyed to a forced mixer to be mixed, and after the powder materials are uniformly mixed, water is added to be mixed into a semi-dry material with certain forming performance.
4. Shaping of
And forming the semi-dry material into a semi-finished product with a certain shape by adopting a hydraulic press.
5. Firing into
And calcining the semi-finished product at high temperature to obtain the mullite porous ceramic product.
Test example 1 binding agent screening test
Aluminate cement and water glass are respectively used as a bonding agent for testing, the influence of the bonding agent on the bending strength is investigated, and the test results are shown in table 1.
Table 1 additive binding agent screening assay
| Formulation No. 1 | 2# formulation | |
| Name of raw materials | Ratio/% of | Ratio/% of |
| Quartz sand powder | 25 | 25 |
| Special-grade bauxite powder | 75 | 75 |
| Aluminate cement (plus) | 5 | |
| Water glass (external) | 5 | |
| Carborundum powder (plus) | 5 | 5 |
| Water (addition) | 6 | 6 |
| Bending strength (MPa) | 4.5 | 3 |
As can be seen from Table 1, the bending strength of the water glass is increased more by adding the aluminate cement, and the aluminate cement is selected as the binder.
Test example 2 mineralizing agent screening test
Titanium dioxide and zirconium dioxide are respectively used as mineralizers for testing, the influence of the mineralizers on the bending strength is investigated, and the test results are shown in table 2.
TABLE 2 screening test with addition of mineralizer
| 3# formulation | 4# formulation | |
| Name of raw materials | Ratio/% of | Ratio/% of |
| Quartz sand powder | 25 | 25 |
| Special-grade bauxite powder | 75 | 75 |
| Aluminate cement (plus) | 5 | 5 |
| Carborundum powder (plus) | 5 | 5 |
| Titanium dioxide (external) | 7 | |
| Zirconium dioxide (addition) | 7 | |
| Water (addition) | 6 | 6 |
| Bending strength (MPa) | 6 | 4 |
As can be seen from Table 2, the bending strength of the added titanium dioxide is increased more than that of the added zirconium dioxide, and the titanium dioxide is selected as a mineralizer.
Test example 3 pore-forming agent screening test
Silicon carbide powder, starch, graphite powder and wood dust are respectively used as pore-forming agents to carry out tests, the influence of the pore-forming agents on the apparent porosity is investigated, and the test results are shown in table 3.
TABLE 3 screening test with pore-forming agent addition
| 5# formulation | 6# formulation | 7# formulation | 8# formulation | |
| Name of raw materials | Ratio/% of | Ratio/% of | Ratio/% of | Ratio/% of |
| Quartz sand powder | 25 | 25 | 25 | 25 |
| Special-grade bauxite powder | 75 | 75 | 75 | 75 |
| Aluminate cement (plus) | 5 | 5 | 5 | 5 |
| Titanium dioxide (external) | 7 | 7 | 7 | 7 |
| Carborundum powder (plus) | 5 | |||
| Starch (addition) | 4 | |||
| Graphite powder (external) | 4 | |||
| Wood flour (external) | 4 | |||
| Water (addition) | 6 | 6 | 6 | 6 |
| Apparent porosity/% | 32 | 33 | 34 | 35 |
As can be seen from Table 3, the apparent porosity of the porous material is 32-35% when different pore formers are added. According to the requirements in the general technical conditions (GBT16533-1996) standards of porous ceramics, the apparent porosity is required to be more than or equal to 30%. The added silicon carbide, starch, graphite powder and wood chips can meet the requirement of apparent porosity in the porous ceramic standard, and the wood chips can be preferentially selected as the pore-forming agent in consideration of the lowest production cost of the wood chips.
Example 1
(1) Abrasive and furnish
Firstly, grinding special-grade alumina and quartz into particles with the particle size less than or equal to 0.088mm by using a ball mill, and then accurately weighing the ground special-grade alumina powder, the ground quartz sand powder, the aluminate cement, the titanium pigment and the wood dust according to the formula shown in the table 4.
(2) Mixing
The weighed materials are firstly dry-mixed for 5-8 minutes by adopting a forced stirrer, and then 6 percent of water is added for wet mixing for 3-5 minutes, so that the mixed materials are ensured to have good forming performance.
(3) Press forming
The mixed material is poured into a mould (the size of the mould is designed according to the shape requirement provided by a user), so that the mould is uniformly filled. Pressing and molding by adopting a hydraulic press, and naturally curing for 24 hours after demolding.
(4) Firing at high temperature
Putting the sample into a sintering furnace for sintering, heating the sample to 1300 ℃ at room temperature, and heating the sample at the temperature of 10 ℃/min; the high temperature point is controlled at 1300 ℃, and the heat preservation time is 4 hours; cooling the mixture to room temperature at 1300 ℃, cooling the mixture according to the temperature of 10 ℃/min, and cooling the mixture to obtain the mullite porous ceramic product.
(5) Index detection
The mullite porous ceramic product is detected according to a test method of the bending strength of a ceramic material GB/T4741-1999 and a test method of the apparent porosity of a ceramic material GB/T3810.3-1999, wherein the bending strength is 6.5MPa, and the apparent porosity is 36%.
TABLE 4 mullite-producing ratio of porous ceramics
| Name of raw materials | Ratio/% of |
| Quartz sand powder | 25 |
| Special-grade bauxite powder | 75 |
| Aluminate cement (plus) | 5 |
| Wood flour (external) | 5 |
| Titanium dioxide (external) | 7 |
| Water (addition) | 6 |
Example 2
(1) Abrasive and furnish
Firstly, grinding special-grade alumina and quartz into particles with the particle size less than or equal to 0.088mm by using a ball mill, and then accurately weighing the ground special-grade alumina powder, the ground quartz sand powder, the aluminate cement, the titanium pigment and the wood dust according to the formula shown in the table 5.
(2) Mixing
The weighed materials are firstly dry-mixed for 5-8 minutes by adopting a forced stirrer, and then 6 percent of water is added for wet mixing for 3-5 minutes, so that the mixed materials are ensured to have good forming performance.
(3) Press forming
The mixed material is poured into a mould (the size of the mould is designed according to the shape requirement provided by a user), so that the mould is uniformly filled. Pressing and molding by adopting a hydraulic press, and naturally curing for 24 hours after demolding.
(4) Firing at high temperature
Putting the sample into a sintering furnace for sintering, heating the sample to 1300 ℃ at room temperature, and heating the sample at the temperature of 10 ℃/min; the high temperature point is controlled at 1300 ℃, and the heat preservation time is 4 hours; heating to room temperature at 1300 ℃, cooling at 10 ℃/min, and cooling to obtain the mullite porous ceramic product.
(5) Index detection
The mullite porous ceramic product is detected according to a test method of the bending strength of a ceramic material GB/T4741-1999 and a test method of the apparent porosity of a ceramic material GB/T3810.3-1999, wherein the bending strength is 7.5MPa, and the apparent porosity is 35%.
TABLE 5 mullite ratio in porous ceramics production
| Name of raw materials | Ratio/% of |
| Quartz sand powder | 25 |
| Special-grade bauxite powder | 75 |
| Aluminate cement (plus) | 7 |
| Wood flour (external) | 5 |
| Titanium dioxide (external) | 8 |
| Water (addition) | 6 |
Claims (10)
1. The preparation method of the mullite porous ceramic is characterized by comprising the following steps: the method comprises the following steps: uniformly mixing quartz sand powder, special-grade bauxite powder, a bonding agent, a mineralizer and a pore-forming agent, adding water, and uniformly mixing to obtain a semi-dry material; pouring the semi-dry material into a mould to form a semi-finished product, and calcining the semi-finished product to obtain mullite porous ceramic; the binding agent is aluminate cement, and the mineralizer is titanium dioxide.
2. The method for preparing mullite porous ceramic according to claim 1, wherein: the pore-forming agent is at least one of silicon carbide, starch, graphite powder, wood chips or plant fibers; furthermore, the addition amount of the pore-forming agent is 5-8% of the total mass of the quartz sand powder and the special-grade bauxite powder.
3. The method for preparing mullite porous ceramic according to claim 1 or 2, wherein: SiO in the quartz sand2More than or equal to 98 percent; al in the special-grade bauxite powder2O3≥85％。
4. The method for preparing mullite porous ceramic according to any one of claims 1 to 3, wherein: the granularity of the quartz sand powder is less than or equal to 0.088 mm; the granularity of the special-grade bauxite powder is less than or equal to 0.088 mm.
5. The method for preparing mullite porous ceramic according to any one of claims 1 to 4, wherein: the addition amount of the aluminate cement is 5-8% of the total mass of the quartz sand powder and the special-grade bauxite powder.
6. The method for preparing mullite porous ceramic according to any one of claims 1 to 5, wherein: the addition amount of the titanium dioxide is 5-8% of the total mass of the quartz sand powder and the special-grade bauxite powder.
7. The method for preparing mullite porous ceramic according to any one of claims 1 to 6, wherein: the addition amount of the water is 6-9% of the total mass of the quartz sand powder and the special-grade bauxite powder.
8. The method for preparing the mullite porous ceramic according to any one of claims 1 to 7, wherein: the water content of each raw material is below 2 percent.
9. The method for preparing mullite porous ceramic according to any one of claims 1 to 8, wherein: the molding pressure is 15-25 MPa, and the pressure is maintained for 5-10 s.
10. The method for preparing mullite porous ceramic according to any one of claims 1 to 9, wherein: the calcining temperature is 1250-1350 ℃, and the time is 3-6 h; preferably, the temperature and time of the calcination is 1300 ℃ x 4 h.
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| CN113754456A (en) * | 2021-11-09 | 2021-12-07 | 长沙中瓷新材料科技有限公司 | Mullite-based ceramic material and preparation method thereof |
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